EP0545297B1 - Receptacle with cap - Google Patents

Receptacle with cap Download PDF

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Publication number
EP0545297B1
EP0545297B1 EP92120267A EP92120267A EP0545297B1 EP 0545297 B1 EP0545297 B1 EP 0545297B1 EP 92120267 A EP92120267 A EP 92120267A EP 92120267 A EP92120267 A EP 92120267A EP 0545297 B1 EP0545297 B1 EP 0545297B1
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EP
European Patent Office
Prior art keywords
vessel
closure
assembly according
sealing
sealing surface
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP92120267A
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German (de)
French (fr)
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EP0545297A1 (en
Inventor
Dieter Dr. Husar
Karl Baldszun
Oliver Beer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eppendorf SE
Original Assignee
Eppendorf Netheler Hinz GmbH
Eppendorf Geraetebau Netheler and Hinz GmbH
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Publication of EP0545297A1 publication Critical patent/EP0545297A1/en
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Publication of EP0545297B1 publication Critical patent/EP0545297B1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D41/00—Caps, e.g. crown caps or crown seals, i.e. members having parts arranged for engagement with the external periphery of a neck or wall defining a pouring opening or discharge aperture; Protective cap-like covers for closure members, e.g. decorative covers of metal foil or paper
    • B65D41/02—Caps or cap-like covers without lines of weakness, tearing strips, tags, or like opening or removal devices
    • B65D41/04—Threaded or like caps or cap-like covers secured by rotation
    • B65D41/0407—Threaded or like caps or cap-like covers secured by rotation with integral sealing means
    • B65D41/0414—Threaded or like caps or cap-like covers secured by rotation with integral sealing means formed by a plug, collar, flange, rib or the like contacting the internal surface of a container neck

Definitions

  • the invention relates to a lid vessel according to the preamble of claim 1.
  • the invention is particularly aimed at lid vessels for laboratory use at extreme temperatures, which have a nominal volume of the order of up to a few milliliters.
  • Conventional vessels are predominantly designed as screw cap vessels and are provided with a separate sealing element in the form of an O-ring. This can result in contamination of the contents of the vessel if the contents of the O-rings are attacked by the ingredients. Furthermore, the additional sealing element causes special manufacturing costs.
  • the screw cover is provided on the bottom with a sealing lip which has the shape of an elongated parabola in longitudinal section.
  • the sealing lip On its circumference, the sealing lip has a lip sealing surface which, when the lid is screwed on, presses elastically against an inner edge of the mouth of the vessel.
  • the front and inner walls of the housing meet practically seamlessly, i.e. the radius of curvature of the inner edge in a longitudinal section plane approaches zero.
  • the lip sealing surface is therefore subjected to a continuous line load, which is accompanied by high surface pressures. These surface pressures mean that the sealing lip in the screwed state is bent considerably inwards compared to its unscrewed position.
  • a screw closure is known in which a stopper with a conical sealing surface is screwed from an initial position so deep into the neck of a bottle made of elastic material that particularly high surface pressures and elastic deformations occur.
  • FR-A-1 153 553 also relates to a larger bottle, in which the sealing of the lid presupposes a considerable deformation of the sealing elements.
  • the bottle stopper is said to have a considerable radial one thanks to a hollow spherical cap made of polyethylene etc. at the bottom of the cap Pressure on the inner surface of the bottle neck for elastic radial deformability can be achieved.
  • the object of the invention is to provide an improved lid vessel of the type mentioned at the outset, which has improved tightness over a wide temperature range from in particular minus 196 ° C. to plus 100 ° C. over a required sealing time of, for example, 20 minutes.
  • the invention proceeds from the surprising Knowledge from the fact that a low surface pressure in the sealing surfaces in the intended temperature range can on the one hand be sufficient for a sufficient sealing effect and on the other hand cause such a small plastic material deformation over the required sealing time that the sealing effect does not drop to unacceptable values and always a minimum tightness that is considered necessary is made available.
  • This approach takes a different path from the known sealing techniques, which assume the need for high surface pressure for a secure seal.
  • the low surface pressure is achieved by a suitable choice of the radii of curvature of the lip sealing surface and the vessel sealing surface in a longitudinal section through the lid container.
  • a sealing lip stiffness also contributes, in which the sealing lip is only subjected to slight elastic deformation under surface pressure, but in particular is sufficient for adjusting the sealing force and for error compensation. As a result, the rate of deformation of the sealing lip is further reduced in the stress situations of interest.
  • the appropriate sealing lip stiffness is achieved in particular through shape and material properties.
  • the sealing lip can be given a compact shape, for example by maximally increasing its width Base corresponds.
  • a trapezoidal shape of the sealing lip cross section can have a favorable influence on the deformation behavior.
  • an acute angle of inclination of the lip sealing surface away from the lid base towards the longitudinal axis of the vessel results in improved error compensation and an increased adjustment path for the surface pressure due to radial lip deformation.
  • the lid base is preferably stiffened against deflection as a result of sealing surface contact or pressure load in order to counteract any lifting of the lip sealing surface from the vessel sealing surface which may be promoted by material flow in the lid base.
  • the lid base preferably has a large wall thickness. If necessary, a wall thickness can be below a limit for piercing a needle tip, which can be determined for conventional piercing devices. If a flat lid contour is not required, a weaker, weaker lid contour can be selected.
  • An undesirable flow of material while reducing the sealing effect can also be counteracted by an annular body which surrounds the housing wall near the housing sealing surface without a gap and can be formed in one piece with the housing or separately from it.
  • the locking elements are preferably inside on a ceiling jacket and outside on a vessel wall and thus from Ingredients of the vessel are arranged away.
  • the locking elements preferably have screw threads which enable fine metering of the surface pressure.
  • the locking is simplified while maintaining the fine metering if the locking elements have snap elements for pre-snapping.
  • the screw threads can be multi-start and have one of the multi-start screw threads each flattened over a fraction of a thread start sections as snap elements for pushing the other screw thread.
  • the initial part of the multi-start thread near the mouth opening is thus used for snapping and the more distant thread sections for screwing.
  • the sealing lip preferably projects in the longitudinal direction of the lid vessel beyond the lid jacket, as a result of which it is easier to insert it into the mouth opening.
  • a vessel according to the invention can consist of a polyolefin such as polypropylene or polyethylene, combinations of different polyolefins for the lid and vessel also being possible.
  • a polyolefin such as polypropylene or polyethylene
  • fluoropolymers such as polytetrafluoroethylene can also be considered, particularly when very aggressive substances are to be filled in.
  • reasons of stiffening the sealing lip and lid base can make it advisable that the lid has a greater modulus of elasticity than the vessel. This can be achieved through the selection of suitable plastics but also through various settings of the plastics, for example by means of additives.
  • the vessel can be used in particular as a safety vessel (centrifugation), for sample storage / sample transport, as a cryogenic vessel and for denaturing protein at 100 ° C in a water bath.
  • FIG. 1 to 3 show a vessel 1 of a lid vessel according to the invention, the filling volume of 1.3 ml of which has a tapering bottom section 2 and a cylindrical main section 3.
  • a vessel wall 4 is provided with fill level marks 5 in the area of these sections 2, 3.
  • the vessel has a screw socket 6, which carries a two-start thread 7.
  • the thread starts 8 ', 8' 'of the two threads on the circumference of the threaded connector 6 are offset by 90 °.
  • the figures show that the initial sections 9 ', 9' 'of a threaded section 6 are flattened and only the subsequent threaded sections 10', 10 '' have a pronounced sawtooth profile over half the circumference of the threaded connector 6.
  • the threaded connector 6 works together with a cover 11 according to FIGS. 4 and 5, the cover base 12 of which carries a cylindrical cover jacket 13 on the circumference.
  • the inside of the cover jacket 13 is provided with a two-start screw thread 14, the saw tooth profile of which is formed uniformly from the beginning of the thread to the end of the thread.
  • the cover 12 is with initial areas of its two threads on the initial sections 9 ', 9''of the screw thread 7 of the vessel 1 can be snapped and can then be screwed onto the threaded sections 10 ′, 10 ′′ provided with a full sawtooth profile for the purpose of further locking.
  • the lid 12 Before the lid 12 is screwed on, it can be captively attached to the vessel 1 by means of a laterally formed, flexible tab 15 by anchoring a tab eyelet 16 with an expansion area 17 in an outer vessel groove 18. Under the vessel groove 18, the vessel 1 has an integrally formed ring body 19, which serves in particular as a support for the tab eye 16 and as a stop for the screwed cover.
  • a concentric sealing lip 20 extends from the lid base 12, which has a compact trapezoidal shape in longitudinal section.
  • the outer flanks of the trapezoid 20 form lip sealing surfaces 21 which, starting from the lid base 12, is inclined at an angle of 25 ° to the central longitudinal axis of the lid 11. In cross section, the radius of curvature of the lip sealing surface 21 goes towards infinity.
  • the sealing lip 20 interacts with a vessel sealing surface 23 which, according to FIGS. 3 and 6, is formed on the inner edge of a vessel mouth 24.
  • the vessel sealing surface has Cross section a radius of curvature of 1 mm.
  • FIGS. 7 to 9 Details of the sealing elements and the interaction with the screw thread are explained with reference to FIGS. 7 to 9. However, these figures do not show any embodiment according to the subject-matter of claim 1, as they do not have a sealing surface with a radius of curvature of 1 mm. They show the dot-dash line of the vessel 1 after the lid 11 has been screwed on before an excess pressure is built up inside as a result of an increase in temperature, and the contours of the lid vessel in solid lines at an overpressure after about 20 minutes of closure time.
  • Fig. 7 shows that the lid base 12 bulges outwards due to the flow of material when pressurized, which is accompanied by a slight change in position of the lip sealing surface 21 and vessel sealing surface 23. Nevertheless, a satisfactory sealing effect can already be observed, because the radii of curvature of the sealing surfaces 21, 23 cause a low surface pressure, which, supported by the slight pre-deformation of the sealing lip 20, results in a low material deformation. In addition, the material deformation in the area of the sealing elements is hindered by an annular body 25, which is formed in one piece with the cover jacket 13 and supports the outside of the vessel wall 4 near the vessel mouth 24.
  • the bulging of the lid base 12 is due of an internal pressure is generally reduced by its greater wall thickness, which is accompanied by less impairment of the seal on the lip sealing surface 21 and the vessel sealing surface 23.
  • the impairment of the sealing seat is still relatively large, because a material with an elastic modulus of 250 N / mm 2 was used as a basis for the cover 11 and an elastic modulus of 500 N / mm 2 for the vessel 1.
  • the E modules were interchanged with the same wall thickness of the cover base 12, ie a value of 500 N / mm 2 was assigned to the cover 11 and a value of 250 N / mm 2 was assigned to the housing 1. As a result, there was significantly less bulging of the lid base 12 and deformation of the sealing surfaces 21, 23.
  • the deformation behavior according to FIGS. 7 to 9 was calculated according to the FEM (finite element method), the material behavior of a polyolefin being used as a basis.
  • FEM finite element method
  • a loss rate of 1.3% i.e. less than 3.9 mg fluid loss

Abstract

A receptacle with cap, which receptacle with cap is made of flexible plastic, in particular for laboratory use under extreme temperatures, in which detachable locking devices act between cap (26) and receptacle (33), a concentric sealing lip (30) which starts from the cap base (29), engages in a receptacle orifice (37) and bears in a sealing manner against a receptacle sealing surface (39) of a receptacle wall (36) is to be reliably sealed over an extreme temperature range, in particular from minus 196 DEG C to plus 100 DEG C. To this end, it is proposed in particular that the sealing lip (30) have a length promoting a pressing of its lip sealing surface (31) against the housing sealing surface (39) under the vapour pressure of enclosed substances. <IMAGE>

Description

Gegenstand der Erfindung ist ein Deckelgefäß nach dem Oberbegriff des Anspruches 1.The invention relates to a lid vessel according to the preamble of claim 1.

Die Erfindung zielt insbesondere auf Deckelgefäße für den Laboreinsatz bei extremen Temperaturen ab, die ein Nennvolumen in der Größenordnung von bis zu wenigen Millilitern aufweisen. Herkömmliche Gefäße sind vorwiegend als Schraubdeckelgefäße ausgebildet und mit einem separaten Dichtungselement in der Form eines O-Ringes versehen. Das kann Verunreinigungen der Gefäßinhalte zur Folge haben, wenn das Material der O-Ringe von den Inhaltsstoffen angegriffen wird. Ferner verursacht das zusätzliche Dichtungselement besondere Fertigungskosten.The invention is particularly aimed at lid vessels for laboratory use at extreme temperatures, which have a nominal volume of the order of up to a few milliliters. Conventional vessels are predominantly designed as screw cap vessels and are provided with a separate sealing element in the form of an O-ring. This can result in contamination of the contents of the vessel if the contents of the O-rings are attacked by the ingredients. Furthermore, the additional sealing element causes special manufacturing costs.

Bei einem vorbekannten Deckelgefäß der eingangs genannten Art ist der Schraubdeckel bodenseitig mit einer Dichtlippe versehen, die im Längsschnitt die Form einer gestreckten Parabel hat. An ihrem Umfang hat die Dichtlippe eine Lippendichtfläche, die bei verschraubtem Deckel elastisch dichtend gegen einen Innenrand der Gefäßmündung drückt. Am Innenrand stoßen Gehäusestirnwand und Gehäuseinnenwand praktisch übergangslos senkrecht aneinander, d.h. der Krümmungsradius des Innenrandes in einer Längsschnittebene geht gegen Null. Die Lippendichtfläche ist somit einer ringsumlaufenden Linienbelastung unterworfen, die mit hohen Flächenpressungen einhergeht. Diese Flächenpressungen bedingen, daß die Dichtlippe im verschraubten Zustand ganz erheblich gegenüber ihrer unverschraubten Lage einwärts gebogen ist.In a previously known cover vessel of the type mentioned at the beginning, the screw cover is provided on the bottom with a sealing lip which has the shape of an elongated parabola in longitudinal section. On its circumference, the sealing lip has a lip sealing surface which, when the lid is screwed on, presses elastically against an inner edge of the mouth of the vessel. At the inner edge, the front and inner walls of the housing meet practically seamlessly, i.e. the radius of curvature of the inner edge in a longitudinal section plane approaches zero. The lip sealing surface is therefore subjected to a continuous line load, which is accompanied by high surface pressures. These surface pressures mean that the sealing lip in the screwed state is bent considerably inwards compared to its unscrewed position.

Bei Raumtemperatur ist dieses Dichtungsverhalten des vorbekannten Gefäßes relativ unproblematisch. Wird das Gefäß jedoch in einem weiten Temperaturbereich von z.B. minus 196°C bis plus 100°C verwendet, kommt es während der erforderlichen Verschlußdauer zu erhöhten Anforderungen. Insbesondere bei den höheren Temperaturen stellt sich eine hohe Materialverformung ein, die zu einer schnellen Deformation der Dichtungsanordnung unter Reduktion der Dichtkraft bis zu einem unzureichenden Wert führt. Dann kann das Gefäß erhebliche Teile des Probenvolumens verlieren. Diese Vorgänge werden durch den erhöhten Dampfdruck der Proben bei den hohen Temperaturen unterstützt, die beim Kochen im Wasserbad 100°C erreichen. Niedrige Temperaturen von beispielsweise 196°C bei flüssigem Stickstoff als Kühlmedium führen zu einer plastischen Kaltverformung des Kunststoffgefäßes insbesondere im vorgespannten Dichtungsbereich mit einhergehender Undichtigkeit. Dabei kann es zur Aufnahme des Kühlmediums kommen, welches nach der erforderlichen Verschlußdauer verdampfen und ein Abplatzen des Deckels bewirken kann. Herausgeschleudertes Probenvolumen führt zu einer Kontamination der Umgebung.At room temperature, this sealing behavior of the previously known vessel is relatively unproblematic. However, if the container is used in a wide temperature range from, for example, minus 196 ° C to plus 100 ° C, there are increased requirements during the required sealing time. In particular at the higher temperatures, a high material deformation occurs, which leads to a rapid deformation of the sealing arrangement while reducing the sealing force to an inadequate value. Then can the vessel will lose significant portions of the sample volume. These processes are supported by the increased vapor pressure of the samples at the high temperatures that reach 100 ° C when boiled in a water bath. Low temperatures of, for example, 196 ° C. with liquid nitrogen as the cooling medium lead to plastic cold deformation of the plastic vessel, in particular in the prestressed sealing area, with an associated leak. This can result in the absorption of the cooling medium, which can evaporate after the required sealing time and cause the cover to flake off. Thrown out sample volume leads to contamination of the environment.

Aus der FR-A-1 487 412 ist ein Schraubverschluß bekannt, bei dem ein Stopfen mit einer konischen Dichtfläche ausgehend von einer Anfangsstellung so tief in den Hals einer Flasche aus elastischem Material geschraubt wird, daß besonders hohe Flächenpressungen und elastische Verformungen eintreten.From FR-A-1 487 412 a screw closure is known in which a stopper with a conical sealing surface is screwed from an initial position so deep into the neck of a bottle made of elastic material that particularly high surface pressures and elastic deformations occur.

Auch die FR-A-1 153 553 betrifft eine größere Flasche, bei der die Abdichtung des Deckels jeweils eine erhebliche Verformung der Dichtelemente voraussetzt. Bei dem Flaschenverschluß soll nämlich durch eine hohle Kalotte aus Polyethylen usw. am Boden der Kappe ein beträchtlicher radialer Druck auf die Innenoberfläche des Flaschenhalses für eine elastische radiale Verformbarkeit erreicht werden.FR-A-1 153 553 also relates to a larger bottle, in which the sealing of the lid presupposes a considerable deformation of the sealing elements. The bottle stopper is said to have a considerable radial one thanks to a hollow spherical cap made of polyethylene etc. at the bottom of the cap Pressure on the inner surface of the bottle neck for elastic radial deformability can be achieved.

Diese Flaschenverschlüsse versagen aus den genannten Gründen bei Einsatz in einem weiten Temperaturbereich.For the reasons mentioned, these bottle caps fail when used in a wide temperature range.

Davon ausgehend liegt der Erfindung die Aufgabe zugrunde, ein verbessertes Deckelgefäß der eingangs genannten Art zu schaffen, das über einen weiten Temperaturbereich von insbesondere minus 196°C bis plus 100°C über eine erforderliche Verschlußdauer von beispielsweise 20 Minuten eine verbesserte Dichtigkeit aufweist.Based on this, the object of the invention is to provide an improved lid vessel of the type mentioned at the outset, which has improved tightness over a wide temperature range from in particular minus 196 ° C. to plus 100 ° C. over a required sealing time of, for example, 20 minutes.

Diese Aufgabe wird durch ein Deckelgefäß mit den Merkmalen des Anspruchs 1 gelöst. Vorteilhafte Ausgestaltungen des Deckelgefäßes sind den Unteransprüchen angegeben.This object is achieved by a lid vessel with the features of claim 1. Advantageous configurations of the lid vessel are specified in the subclaims.

Die Erfindung geht von der überraschenden Erkenntnis aus, daß eine geringe Flächenpressung in den Dichtflächen in dem beabsichtigten Temperaturbereich einerseits für eine ausreichende Dichtwirkung ausreichen kann und andererseits über die erforderliche Verschlußdauer hinweg eine so geringe plastische Materialverformung verursacht, daß die Dichtwirkung nicht auf unzuträgliche Werte absinkt und stets eine für notwendig gehaltene Mindestdichtigkeit zur Verfügung gestellt wird. Dieser Ansatz beschreitet gegenüber den bekannten Dichttechniken einen anderen Weg, die von der Notwendigkeit einer hohen Flächenpressung für eine sichere Abdichtung ausgehen. Erreicht wird die geringe Flächenpressung durch geeignete Wahl der Krümmungsradien von Lippendichtfläche und Gefäßdichtfläche in einem Längsschnitt durch das Deckelgefäß.The invention proceeds from the surprising Knowledge from the fact that a low surface pressure in the sealing surfaces in the intended temperature range can on the one hand be sufficient for a sufficient sealing effect and on the other hand cause such a small plastic material deformation over the required sealing time that the sealing effect does not drop to unacceptable values and always a minimum tightness that is considered necessary is made available. This approach takes a different path from the known sealing techniques, which assume the need for high surface pressure for a secure seal. The low surface pressure is achieved by a suitable choice of the radii of curvature of the lip sealing surface and the vessel sealing surface in a longitudinal section through the lid container.

Grundsätzlich erfüllt man die Forderung nach einer möglichst geringen Flächenpressung,wenn beide Krümmungsradien gegen Unendlich gehen, d.h. Lippendichtfläche und Gefäßdichtfläche im Längsschnitt Linienberührung haben. Eine solche Dichtanordnung ist jedoch in Herstellung und Handhabung problematisch, insbesondere weil geringe Toleranzschwankungen, Unrundheiten oder Verletzungen der Dichtflächen eine Undichtigkeit zur Folge haben. Erfindungsgemäß geht nur einer der Krümmungsradien gegen Unendlich. Der andere Krümmungsradius ist geringer, nämlich etwa 1 mm. Mit dieser Radienkombination wird eine geringe Flächenpressung erreicht und ein Ausgleich von Ungenauigkeiten oder Verletzungen durch geringfügige Verformung insbesondere der Dichtfläche mit dem geringeren Krümmungsradius erreicht. Letzterer wird bevorzugt an der Gehäusedichtfläche ausgebildet, wo Verletzungen am ehesten zu besorgen sind. Befindet sich die Gehäusedichtfläche am Innenrand der Gefäßmündung, ist ein verbesserter Schutz vor Verletzungen und Kontamination gegeben.Basically, the requirement for the lowest possible surface pressure is met if both radii of curvature go towards infinity, ie lip sealing surface and vessel sealing surface have linear contact in longitudinal section. However, such a sealing arrangement is problematic in manufacture and handling, in particular because small tolerance fluctuations, out-of-roundness or injuries to the sealing surfaces result in a leak. According to the invention, only one of the radii of curvature goes against Infinite. The other radius of curvature is smaller, namely about 1 mm. With this combination of radii, a low surface pressure is achieved and inaccuracies or injuries are compensated for by slight deformation, in particular of the sealing surface with the smaller radius of curvature. The latter is preferably formed on the housing sealing surface, where injuries are most likely to be worried. If the housing sealing surface is located on the inner edge of the vessel mouth, there is improved protection against injuries and contamination.

Zur Verringerung der Materialverformung bei extremen Temperaturen trägt außerdem eine Dichtlippensteifigkeit bei, bei der die Dichtlippe unter Flächenpressung einen nur geringen, jedoch insbesondere für eine Einstellung der Dichtkraft und einen Fehlerausgleich ausreichenden elastischen Verformung unterworfen ist. Hierdurch wird die Deformationsgeschwindigkeit der Dichtlippe in den interessierenden Beanspruchungssituationen weiter herabgesenkt. Erreicht wird die geeignete Dichtlippensteifigkeit insbesondere durch Formgebung und Materialbeschaffenheit. Hierzu kann der Dichtlippe eine gedrungene Form gegeben werden, beispielsweise indem ihre Höhe maximal der Breite ihrer Basis entspricht. Ferner kann eine Trapezform des Dichtlippenquerschnittes das Verformungsverhalten günstig beeinflussen. Überdies bewirkt ein spitzer Neigungswinkel der Lippendichtfläche vom Deckelboden weg zur Längsachse des Gefäßes hin einen verbesserten Fehlerausgleich und einen vergrößerten Einstellweg für die Flächenpressung infolge radialer Lippenverformung.To reduce the material deformation at extreme temperatures, a sealing lip stiffness also contributes, in which the sealing lip is only subjected to slight elastic deformation under surface pressure, but in particular is sufficient for adjusting the sealing force and for error compensation. As a result, the rate of deformation of the sealing lip is further reduced in the stress situations of interest. The appropriate sealing lip stiffness is achieved in particular through shape and material properties. For this purpose, the sealing lip can be given a compact shape, for example by maximally increasing its width Base corresponds. Furthermore, a trapezoidal shape of the sealing lip cross section can have a favorable influence on the deformation behavior. In addition, an acute angle of inclination of the lip sealing surface away from the lid base towards the longitudinal axis of the vessel results in improved error compensation and an increased adjustment path for the surface pressure due to radial lip deformation.

Bevorzugt ist der Deckelboden gegen Ausbiegung infolge Dichtflächenanlage oder Druckbelastung versteift, um einem gegebenenfalls durch Materialfluß im Deckelboden geförderten Abheben der Lippendichtfläche von der Gefäßdichtfläche entgegenzuwirken. Bevorzugt hat hierzu der Deckelboden eine große Wandstärke. Bei Erfordernis kann eine Wandstärke unterhalb einer Grenze für das Durchstechen einer Nadelspitze liegen, die für gebräuchliche Durchstechvorrichtungen ermittelbar ist. Bei Nichterfordernis einer ebenen Deckelkontur kann eine eingezogene schwächere Deckelkontur gewählt werden.The lid base is preferably stiffened against deflection as a result of sealing surface contact or pressure load in order to counteract any lifting of the lip sealing surface from the vessel sealing surface which may be promoted by material flow in the lid base. For this purpose, the lid base preferably has a large wall thickness. If necessary, a wall thickness can be below a limit for piercing a needle tip, which can be determined for conventional piercing devices. If a flat lid contour is not required, a weaker, weaker lid contour can be selected.

Einem unerwünschten Materialfluß unter Verringerung der Dichtwirkung kann ferner durch einen Ringkörper entgegengewirkt werden, der die Gehäusewand nahe der Gehäusedichtfläche spaltfrei umgibt und einteilig mit dem Gehäuse oder separat von diesem ausgebildet sein kann.An undesirable flow of material while reducing the sealing effect can also be counteracted by an annular body which surrounds the housing wall near the housing sealing surface without a gap and can be formed in one piece with the housing or separately from it.

Die Verriegelungselemente sind bevorzugt innen an einem Deckenmantel und außen an einer Gefäßwand und somit von Inhaltsstoffen des Gefäßes entfernt angeordnet. Bevorzugt weisen die Verriegelungselemente Schraubgewinde auf, die ein feines Dosieren der Flächenpressung ermöglichen. Zugleich wird die Verriegelung unter Erhalt der Feindosierung vereinfacht, wenn die Verriegelungselemente Schnappelemente für eine Vorverschnappung aufweisen. Dafür können die Schraubengewinde mehrgängig sein und eines der mehrgängigen Schraubengewinde jeweils über einen Bruchteil eines Gewindeganges abgeflachte Anfangsabschnitte als Schnappelemente zum Überschieben des anderen Schraubengewindes haben. Der Anfangsteil des mehrgängigen Gewindes nahe der Mündungsöffnung wird somit zum Verschnappen und die weiter entfernten Gewindeabschnitte zum Verschrauben benutzt. Bevorzugt ragt die Dichtlippe in Längsrichtung des Deckelgefäßes über den Deckelmantel hinaus, wodurch ihr Einführen in die Mündungsöffnung erleichtert ist.The locking elements are preferably inside on a ceiling jacket and outside on a vessel wall and thus from Ingredients of the vessel are arranged away. The locking elements preferably have screw threads which enable fine metering of the surface pressure. At the same time, the locking is simplified while maintaining the fine metering if the locking elements have snap elements for pre-snapping. For this purpose, the screw threads can be multi-start and have one of the multi-start screw threads each flattened over a fraction of a thread start sections as snap elements for pushing the other screw thread. The initial part of the multi-start thread near the mouth opening is thus used for snapping and the more distant thread sections for screwing. The sealing lip preferably projects in the longitudinal direction of the lid vessel beyond the lid jacket, as a result of which it is easier to insert it into the mouth opening.

Ein erfindungsgemäßes Gefäß kann aus einem Polyolefin wie Polypropylen oder Polyethylen bestehen, wobei auch Kombinationen verschiedener Polyolefine für Deckel und Gefäß möglich sind. Ferner kommt der Einsatz von Fluorpolymeren wie Polytetrafluorethylen in Betracht, insbesondere wenn sehr aggressive Substanzen eingefüllt werden sollen. Vor allem Gründe der Versteifung von Dichtlippe und Deckelboden können es ratsam erscheinen lassen, daß der Deckel einen größeren E-Modul als das Gefäß hat. Dies kann durch Auswahl geeigneter Kunststoffe aber auch durch verschiedene Einstellungen der Kunststoffe z.B. mittels Zusatzstoffen erreicht werden.A vessel according to the invention can consist of a polyolefin such as polypropylene or polyethylene, combinations of different polyolefins for the lid and vessel also being possible. The use of fluoropolymers such as polytetrafluoroethylene can also be considered, particularly when very aggressive substances are to be filled in. In particular, reasons of stiffening the sealing lip and lid base can make it advisable that the lid has a greater modulus of elasticity than the vessel. This can be achieved through the selection of suitable plastics but also through various settings of the plastics, for example by means of additives.

Erfindungsgemäß wird somit die erforderliche Dichtigkeit unter den gewünschten Bedingungen erreicht, wobei keine zusätzlichen Dichtelemente wie O-Ringe benötigt werden und der damit verbundene Fertigungs- und Montageaufwand sowie Verunreinigungsprobleme entfallen. Das Gefäß ist insbesondere als Sicherheitsgefäß (Zentrifugation), für Probenlagerung/Probentransport, als Kryogefäß und zur Denaturierung von Eiweiß bei 100°C im Wasserbad nutzbar.According to the invention, the required tightness is thus achieved under the desired conditions, no additional sealing elements such as O-rings being required, and the associated manufacturing and assembly work and contamination problems being eliminated. The vessel can be used in particular as a safety vessel (centrifugation), for sample storage / sample transport, as a cryogenic vessel and for denaturing protein at 100 ° C in a water bath.

Weitere Einzelheiten und Vorteile des Gegenstandes der Erfindung ergeben sich aus der nachfolgenden Beschreibung der zugehörigen Zeichnungen, die bevorzugte Ausführungsformen zeigen. In den Zeichnungen zeigen:

Fig. 1 bis 3
ein Gefäß mit Gehäusedichtfläche am Mündungsinnenrand in Seitenansicht, um 90° gedreht und im Längsschnitt;
Fig. 4 und 5
Deckel desselben Gefäßes in vergrößertem Teil-Längsschnitt und in der Draufsicht;
Fig. 6
Mündungsinnenrand desselben Gefäßes gemäß vergrösserter Teilansicht VI der Fig. 3;
Fig. 7
Deckelgefäß gemäß Fig. 1 bis 6 unter Überdruck in einem schematischen Teilschnitt durch den Oberbereich;
Fig. 8
Deckelgefäß mit gegenüber Fig. 7 verstärktem Deckelboden in einem Schnitt entsprechend Fig. 7;
Fig. 9
Deckelgefäß mit gegenüber Fig. 8 veränderter Beschaffenheit von Deckel und Gefäß in einer Darstellung entsprechend Fig. 8.
Further details and advantages of the subject matter of the invention will become apparent from the following description of the accompanying drawings, which show preferred embodiments. The drawings show:
1 to 3
a vessel with a sealing surface on the inner rim of the mouth in side view, rotated by 90 ° and in longitudinal section;
4 and 5
Lid of the same vessel in an enlarged partial longitudinal section and in plan view;
Fig. 6
Inner rim of the same vessel according to enlarged partial view VI of FIG. 3;
Fig. 7
1 to 6 under pressure in a schematic partial section through the upper region;
Fig. 8
Lid vessel with lid bottom reinforced in relation to FIG. 7 in a section corresponding to FIG. 7;
Fig. 9
Lidded vessel with a changed nature of the lid and vessel compared to FIG. 8 in a representation corresponding to FIG. 8.

Die Fig. 1 bis 3 zeigen ein Gefäß 1 eines erfindungsgemässen Deckelgefäßes, dessen Füllvolumen von 1,3 ml einen sich verjüngenden Bodenabschnitt 2 und einen zylindrischen Hauptabschnitt 3 aufweist. Im Bereich dieser Abschnitte 2, 3 ist eine Gefäßwand 4 mit Füllstandsmarken 5 versehen.1 to 3 show a vessel 1 of a lid vessel according to the invention, the filling volume of 1.3 ml of which has a tapering bottom section 2 and a cylindrical main section 3. A vessel wall 4 is provided with fill level marks 5 in the area of these sections 2, 3.

Oben hat das Gefäß einen Schraubstutzen 6, der ein zweigängiges Gewinde 7 trägt. Fig. 1 und 2 ist entnehmbar, daß Gewindeanfänge 8', 8'' der beiden Gewindegänge auf dem Umfang des Gewindestutzens 6 um 90° gegeneinander versetzt sind. Ferner zeigen die Figuren, daß über ein Viertel des Gewindestutzens 6 erstreckte Anfangsabschnitte 9', 9'' der Gewinde abgeflacht ist und erst die sich anschließenden Gewindeabschnitte 10', 10'' über den halben Umfang des Gewindestutzens 6 hinweg ein ausgeprägtes Sägezahnprofil haben.At the top, the vessel has a screw socket 6, which carries a two-start thread 7. 1 and 2 can be seen that the thread starts 8 ', 8' 'of the two threads on the circumference of the threaded connector 6 are offset by 90 °. Furthermore, the figures show that the initial sections 9 ', 9' 'of a threaded section 6 are flattened and only the subsequent threaded sections 10', 10 '' have a pronounced sawtooth profile over half the circumference of the threaded connector 6.

Der Gewindestutzen 6 arbeitet mit einem Deckel 11 gemäß Fig. 4 und 5 zusammen, dessen Deckelboden 12 umfangsseitig einen zylindrischen Deckelmantel 13 trägt. Innen ist der Deckelmantel 13 mit einem zweigängigen Schraubgewinde 14 versehen, dessen Sägezahnprofilierung vom Gewindeanfang bis zum Gewindeende gleichmäßig durchgebildet ist. Der Deckel 12 ist mit Anfangsbereichen seiner beiden Gewindegänge auf die Anfangsabschnitte 9', 9'' des Schraubgewindes 7 des Gefäßes 1 schnappbar und kann dann zwecks weiterer Verriegelung auf die mit einem vollen Sägezahnprofil versehenen Gewindeabschnitte 10', 10'' geschraubt werden.The threaded connector 6 works together with a cover 11 according to FIGS. 4 and 5, the cover base 12 of which carries a cylindrical cover jacket 13 on the circumference. The inside of the cover jacket 13 is provided with a two-start screw thread 14, the saw tooth profile of which is formed uniformly from the beginning of the thread to the end of the thread. The cover 12 is with initial areas of its two threads on the initial sections 9 ', 9''of the screw thread 7 of the vessel 1 can be snapped and can then be screwed onto the threaded sections 10 ′, 10 ″ provided with a full sawtooth profile for the purpose of further locking.

Vor dem Verschrauben des Deckels 12 kann dieser mittels einer seitlich angeformten, flexiblen Lasche 15 unverlierbar am Gefäß 1 befestigt werden, indem eine Laschenöse 16 mit einem Dehnbereich 17 in einer äußeren Gefäßnut 18 verankert wird. Unter der Gefäßnut 18 hat das Gefäß 1 einen angeformten Ringkörper 19, der insbesondere als Auflage für die Laschenöse 16 sowie als Anschlag für die Deckelverschraubung dient.Before the lid 12 is screwed on, it can be captively attached to the vessel 1 by means of a laterally formed, flexible tab 15 by anchoring a tab eyelet 16 with an expansion area 17 in an outer vessel groove 18. Under the vessel groove 18, the vessel 1 has an integrally formed ring body 19, which serves in particular as a support for the tab eye 16 and as a stop for the screwed cover.

Durch Verschraubung des Deckels 12 wird dessen Abdichtung bewirkt. Hierzu geht gemäß Fig. 4 vom Deckelboden 12 eine konzentrische Dichtlippe 20 aus, die im Längsschnitt eine gedrungene Trapezform hat. Die Außenflanken des Trapezes 20 bilden Lippendichtflächen 21, die ausgehend vom Deckelboden 12 um einen Winkel von 25° zur Mittellängsachse des Deckels 11 hin geneigt ist. Im Querschnitt geht der Krümmungsradius der Lippendichtfläche 21 gegen Unendlich.The cover 12 is sealed by screwing it together. For this purpose, according to FIG. 4, a concentric sealing lip 20 extends from the lid base 12, which has a compact trapezoidal shape in longitudinal section. The outer flanks of the trapezoid 20 form lip sealing surfaces 21 which, starting from the lid base 12, is inclined at an angle of 25 ° to the central longitudinal axis of the lid 11. In cross section, the radius of curvature of the lip sealing surface 21 goes towards infinity.

Die Dichtlippe 20 wirkt mit einer Gefäßdichtfläche 23 zusammen, die gemäß Fig. 3 und 6 am Innenrand einer Gefäßmündung 24 ausgebildet ist. Die Gefäßdichtfläche hat im Querschnitt einen Krümmungsradius von 1 mm.The sealing lip 20 interacts with a vessel sealing surface 23 which, according to FIGS. 3 and 6, is formed on the inner edge of a vessel mouth 24. The vessel sealing surface has Cross section a radius of curvature of 1 mm.

Einzelheiten der Dichtelemente und das Zusammenwirken mit dem Schraubgewinde werden anhand der Fig. 7 bis 9 erläutert. Diese Abbildungen zeigen allerdings insoweit keine Ausführungsform nach dem Gegenstand des Anspruchs 1, als bei ihnen eine Dichtfläche mit einem Krümmungsradius von 1 mm nicht vorhanden ist. Sie zeigen strichpunktiert das Gefäß 1 nach dem Aufschrauben des Deckels 11 bevor infolge Temperaturerhöhung ein Überdruck im Inneren aufgebaut ist und in ausgezogenen Linien die Konturen des Deckelgefäßes bei einem Überdruck nach etwa 20 Minuten Verschlußdauer.Details of the sealing elements and the interaction with the screw thread are explained with reference to FIGS. 7 to 9. However, these figures do not show any embodiment according to the subject-matter of claim 1, as they do not have a sealing surface with a radius of curvature of 1 mm. They show the dot-dash line of the vessel 1 after the lid 11 has been screwed on before an excess pressure is built up inside as a result of an increase in temperature, and the contours of the lid vessel in solid lines at an overpressure after about 20 minutes of closure time.

Fig. 7 zeigt, daß sich der Deckelboden 12 infolge des Materialflusses bei Druckbeaufschlagung nach außen wölbt, womit eine geringfügige Lageveränderung der Lippendichtfläche 21 und Gefäßdichtfläche 23 einhergeht. Dennoch ist bereits eine zufriedenstellende Dichtwirkung zu verzeichnen, weil die Krümmungsradien der Dichtflächen 21, 23 eine geringe Flächenpressung verursachen, was unterstützt durch die geringe Vorverformung der Dichtlippe 20 eine geringe Materialverformung bedingt. Zusätzlich behindert wird die Materialverformung im Bereich der Dichtelemente durch einen Ringkörper 25, welcher einteilig mit dem Deckelmantel 13 ausgebildet ist und die Gefäßwand 4 nahe der Gefäßmündung 24 außen abstützt.Fig. 7 shows that the lid base 12 bulges outwards due to the flow of material when pressurized, which is accompanied by a slight change in position of the lip sealing surface 21 and vessel sealing surface 23. Nevertheless, a satisfactory sealing effect can already be observed, because the radii of curvature of the sealing surfaces 21, 23 cause a low surface pressure, which, supported by the slight pre-deformation of the sealing lip 20, results in a low material deformation. In addition, the material deformation in the area of the sealing elements is hindered by an annular body 25, which is formed in one piece with the cover jacket 13 and supports the outside of the vessel wall 4 near the vessel mouth 24.

Gemäß Fig. 8 wird die Auswölbung des Deckelbodens 12 infolge eines Innendruckes durch dessen größere Wandstärke grundsätzlich verringert, womit eine geringere Beeinträchtigung der Abdichtung an Lippendichtfläche 21 und Gefäßdichtfläche 23 einhergeht. Hier ist die Beeinträchtigung des Dichtsitzes noch relativ groß, weil für den Deckel 11 ein Material mit einem E-Modul von 250 N/mm2 und für das Gefäß 1 ein E-Modul von 500 N/mm2 zugrundegelegt wurde.8, the bulging of the lid base 12 is due of an internal pressure is generally reduced by its greater wall thickness, which is accompanied by less impairment of the seal on the lip sealing surface 21 and the vessel sealing surface 23. Here the impairment of the sealing seat is still relatively large, because a material with an elastic modulus of 250 N / mm 2 was used as a basis for the cover 11 and an elastic modulus of 500 N / mm 2 for the vessel 1.

Bei der Ausführungsform in Fig. 9 wurden bei gleicher Wandstärke des Deckelbodens 12 die E-Module vertauscht, d.h. dem Deckel 11 ein Wert von 500 N/mm2 und dem Gehäuse 1 ein Wert von 250 N/mm2 zugeordnet. Infolgedessen war eine deutlich geringere Auswölbung des Deckelbodens 12 sowie Verformung der Dichtflächen 21, 23 zu verzeichnen.In the embodiment in FIG. 9, the E modules were interchanged with the same wall thickness of the cover base 12, ie a value of 500 N / mm 2 was assigned to the cover 11 and a value of 250 N / mm 2 was assigned to the housing 1. As a result, there was significantly less bulging of the lid base 12 and deformation of the sealing surfaces 21, 23.

Das Verformungsverhalten gemäß Fig. 7 bis 9 wurde nach der FEM (Finite Elemente Methode) berechnet, wobei das Materialverhalten eines Polyolefines zugrunde gelegt wurde. Mit erfindungsgemäßen Deckelgefäßen konnten bereits bei 1,3 ml Füllvolumen im Wasserbad bei 100°C und während einer Verschlußdauer von mindestens 30 Minuten unter 0,3 % Verlustrate (d.h. weniger als 3,9 mg Flüssigkeitsverlust) erzielt werden.The deformation behavior according to FIGS. 7 to 9 was calculated according to the FEM (finite element method), the material behavior of a polyolefin being used as a basis. With the lid vessels according to the invention, a loss rate of 1.3% (i.e. less than 3.9 mg fluid loss) could be achieved with a filling volume of 1.3 ml in a water bath at 100 ° C. and for at least 30 minutes.

Claims (17)

  1. A closure vessel assembly made of elastic plastic having a nominal volume of up to several milliliters for use in laboratory work within a range of temperatures between -196°C and +100°C, wherein releasable locking means are effective between a lid (11) and vessel (1), an annular sealing lip (20) integrally connected to the top wall (12) of the lid being insertable into a mouth (24) of the vessel and being axially movable with a lip sealing surface (21) in sealing engagement with a vessel sealing surface (23) on a vessel wall (4), characterized in that for minimum surface pressure and at sufficient sealing performance under consideration of a deformation of the material during the required closing time of the vessel said lip sealing surface (21) and said vessel sealing surface (23) have in a longitudinal cross section radii of curvature, with one of said radii approximating infinity and the other having a value of about 1 mm, and said sealing lip (20) is substantially stiff, and having a small elastic deformability sufficient to obtain the desired sealing force and tolerance compensation.
  2. A closure vessel assembly according to claim 1, characterized in that said vessel sealing surface (23) is provided with the smaller one of said radii of curvature.
  3. A closure vessel assembly according to claim 1 or 2, characterized in that said vessel sealing surface (23) is formed on an internal rim of said mouth (24) of the vessel.
  4. A closure vessel assembly according to any of claims 1 to 3, characterized in that said sealing lip (20) has a height approximately equal to the width of its base.
  5. A closure vessel assembly according to any of claims 1 to 4, characterized in that said sealing lip (20) has a longitudinal cross section of approximately trapezoidal shape.
  6. A closure vessel assembly according to any of claims 1 to 5, characterized in that said lip sealing surface (21) extends from said top wall (12) of the lid under an acute angle of inclination towards a longitudinal central axis.
  7. A closure vessel assembly according to any of claims 1 to 6, characterized in that said top wall (12) of the lid is of substantial stiffness in order to avoid any substantial flexing thereof resulting from sealing surface pressure or superatmospheric pressure in the vessel.
  8. A closure vessel assembly according to claim 7, characterized in that said top wall (12) of the lid is provided with a big wall thickness under a limit for piercing a needle tip through.
  9. A closure vessel assembly according to any of claims 1 to 8, characterized in that said vessel wall (4) is surrounded by an annular member (25) closely adjacent to said vessel sealing surface (23) without any space therebetween.
  10. A closure vessel assembly according to any of claims 1 to 9, characterized in that locking means (7, 14) are provided at an internal side of a closure side wall (13) and on an external side of said vessel wall (4).
  11. A closure vessel assembly according to any of claims 1 to 10, characterized in that said locking means comprise helical threads (7, 14).
  12. A closure vessel assembly according to claim 11, characterized in that said locking means comprise snap-on means (9', 9''; 14) for providing an initial snapping action.
  13. A closure vessel assembly according to any of claims 10 to 12, characterized in that said helical threads (7, 14) are multiple threads and one of said multiple threads has initial portions (9', 9'') of reduced height which each extend along a fraction of a turn of said thread so as to serve as snap-on elements adapted to be brought into snapping engagement with the other helical thread (14).
  14. A closure vessel assembly according to any of claims 10 to 13, characterized in that said sealing lip extends beyond said closure side wall in a longitudinal direction.
  15. A closure vessel assembly according to any of claims 1 to 14, characterized in that the material of the assembly comprises a polyolefin.
  16. A closure vessel assembly according to any of claims 1 to 15, characterized in that the material of the assembly comprises a fluorpolymer.
  17. A closure vessel assembly according to any of claims 1 to 16, characterized in that the closure (11) has a modulus of elasticity which exceeds that of the vessel (1).
EP92120267A 1991-12-03 1992-11-27 Receptacle with cap Expired - Lifetime EP0545297B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4139810A DE4139810C2 (en) 1991-12-03 1991-12-03 Lid jar
DE4139810 1991-12-03

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EP0545297A1 EP0545297A1 (en) 1993-06-09
EP0545297B1 true EP0545297B1 (en) 1997-07-09

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US (1) US5916525A (en)
EP (1) EP0545297B1 (en)
JP (1) JP2802357B2 (en)
AT (1) ATE155102T1 (en)
DE (2) DE4139810C2 (en)
ES (1) ES2104801T3 (en)

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Also Published As

Publication number Publication date
EP0545297A1 (en) 1993-06-09
JPH0679184A (en) 1994-03-22
DE59208682D1 (en) 1997-08-14
ATE155102T1 (en) 1997-07-15
ES2104801T3 (en) 1997-10-16
JP2802357B2 (en) 1998-09-24
DE4139810C2 (en) 1995-03-09
DE4139810A1 (en) 1993-06-09
US5916525A (en) 1999-06-29

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